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Article

Comparison of the Application of High-Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS) and Collision/Reaction Cell Technology of Inductively Coupled Plasma Mass Spectrometry (ICP-CCT-MS) in the Determination of Selenium in Coal-Bearing Strata

by
Shumao Zhao
1,2,*,
Rongkun Jia
1,2,
Qiuchan Han
1,2,
Niande Shang
1,2,
Kaiyan Teng
1,2 and
Jiawei Feng
1,2
1
Key Laboratory of Coalbed Methane Resources and Reservoir Formation Process, Ministry of Education, China University of Mining and Technology, Xuzhou 221008, China
2
School of Resources and Geosciences, China University of Mining and Technology, Xuzhou 221116, China
*
Author to whom correspondence should be addressed.
Minerals 2024, 14(5), 510; https://doi.org/10.3390/min14050510
Submission received: 30 April 2024 / Revised: 7 May 2024 / Accepted: 11 May 2024 / Published: 13 May 2024
(This article belongs to the Special Issue Selenium, Tellurium and Precious Metal Mineralogy)
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Abstract

:
Selenium, a trace element of significant importance for human health and the environment, can be introduced into the environment through coal combustion. Accurate determination of selenium in coal and coal-bearing strata is essential for implementing effective management strategies and control measures to minimize potential risks to human health and the environment. This study introduces an improved approach for the determination of 77Se in the medium resolution mode using HR-ICP-MS, effectively separating interference from doubly charged ions and enabling precise determination of selenium in coal-bearing strata. The relative errors of the standard reference samples obtained by HR-ICP-MS are between 0.65% and 6.33%, comparing to that of ICP-CCT-MS (1.58%–17.27%), prove the reliability of this method. Additionally, the X (bar)—S control charts obtained from HR-ICP-MS compared to ICP-CCT-MS demonstrate the superior stability of HR-ICP-MS in continuous determination. Consequently, though ICP-CCT-MS has better instrumental stability reflected through the internal standard recovery (ICP-CCT-MS:104.81%; HR-ICP-MS:80.54%), HR-ICP-MS is recommended as the preferred method for selenium determination in coal-bearing strata because of its high accuracy and good stability.

1. Introduction

Coal, one of the most important global energy sources, has garnered significant attention in recent years due to the trace element it contains, which has implications for the environment and human health [1,2,3,4,5,6,7]. Among these elements, selenium (Se) plays a vital role in physiological functions for humans and animals when consumed in moderate amounts [8,9,10,11,12]. However, excessive intake of Se can lead to selenosis [13,14,15,16]. Additionally, selenium is environmentally sensitive, and excessive selenium may contaminate water bodies and inhibit plant growth [17,18,19]. During coal combustion, Se can be released into the atmosphere, posing risks to the environment and human beings [20,21,22,23,24,25,26,27,28,29,30,31,32,33]. Therefore, accurate determination of selenium in coal and coal-bearing strata holds great significance for the coal mining industry, environmental protection, and human health.
Various methods have been developed for determining selenium in coal-bearing strata. Traditional methods include atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), and inductively coupled plasma atomic emission spectrometry (ICP-AES) [34,35,36,37,38,39,40,41,42]. While these methods provide a certain degree of accuracy and reliability, they present disadvantages such as complicated sample pre-treatment procedures that result in prolonged and intricate analytical processes, as well as limited sensitivity for detection [37,38,40,42]. However, advancements in science and technology have introduced new determination methods to enhance accuracy and sensitivity. For instance, high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) enables analysis and quantification of selenium morphology in coal [43,44,45,46], providing valuable insights into selenium’s environmental behavior and biological effects. Furthermore, other analytical methods, such as collision/reaction cell technology of inductively coupled plasma mass spectrometry (ICP-CCT-MS) [47,48,49,50,51] and hydride generation atomic fluorescence spectroscopy (HG-AFS) [52,53,54], have also been applied in the determination of selenium in coal-bearing strata.
High-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS), an improved method of ICP-MS, has gained widespread usage in trace element determination in coal-bearing strata [55,56,57,58]. However, limited discussions exist regarding interferences in the testing process of Se and its application in coal-bearing strata [24,51,59,60]. In this study, we conduct a systematic analysis of the suffered interferences of six natural isotopes of Se during mass spectrometry, propose a method for determining 77Se at medium resolution, and evaluate the reliability of this method using standard reference samples. The method is also compared with ICP-CCT-MS to discuss their application for Se determination in coal-bearing strata in terms of accuracy, precision, and stability.

2. Methods and Materials

2.1. Instruments

The instruments used for the comparison of Se determination in coal-bearing strata were an Attom ES HR-ICP-MS (Nu Instruments, Wrexham, UK), equipped with a Teflon sampling system and a quartz torch with a quartz injector tube, and a ThermoFisher ICP-MS (X Series II, Waltham, MA, USA), equipped with an Automated 3rd Generation Collision Cell Technology (CCTED). An UltraClave microwave high-pressure reactor (Milestone, Sorisole, Italy) was used for sample digestion before testing under a load pressure of 50 bar. Ultrapure water (18.2 MΩ·cm), produced by Milli-Q IQ 7010 Ultrapure water system (Millipore, Guyancourt, France), was used in all experiments. A DuoPUR acid purification system (Milestone, Sorisole, Italy) was utilized for further purification of the HNO3 (GR, 65%, v:v). All vessels used in the experiments were cleaned by the TraceCLEAN Automatic Acid Reflux System (Milestone, Sorisole, Italy) at 250 °C for 2.5 h.

2.2. Reagents and Gasses

A series of Se standard solutions consisting of 6 concentration levels (0, 1, 10, 30, 50, and 100 μg/L) were configured from the 100 μg/mL standard reference solution (Inorganic Ventures, CCS4). In order to check the stability of the instrument during testing, the internal standard stock solution was diluted from the 1000 μg/mL Rh reference solution (GSB 04-1746-2004, National Center of Analysis and Testing for Nonferrous Metals and Electronic Materials) to 10 μg/L.
The further purified guaranteed reagent HNO3 (65%, v:v) and the metal–oxide–semiconductor (MOS) reagent HF (40%, v:v) were used for sample digestion. For the cooling, auxiliary, and nebulizer gas, ultrapure argon was used in both HR-ICP-MS and ICP-CCT-MS. In addition, the ultrapure (99.999% pure) mixed gas composed of 93.33% He and 6.67% H2 was introduced as the collision gas in ICP-CCT-MS.

2.3. Investigated Samples

A total of five standard reference materials were chosen to be detected in order to evaluate the accuracy, including two bituminous coal samples (SRM 1632e and SRM 2685c) and two fly ash samples (SRM 1633c and SRM 2691) from the National Institute of Standards and Technology (NIST) and a rock sample (GSR-20) from the National Institute of Metrology, China (NIM). Moreover, a study area with coal-bearing strata from Qisheng mine, Xingtai coal field, was selected to make a comparison between the two methods. A thorough description of all the investigated samples is listed in Table 1.

2.4. Sample Digestion

Five milliliters of purified HNO3 and two milliliters of HF (metal–oxide–semiconductor, MOS) were added to 50 mg of coal samples that were broken to less than 200 mesh, and five milliliters of HF (MOS) and two milliliters of purified HNO3 were added to the non-coal samples, respectively. The samples were then put into the UltraClave reactor for digestion. The microwave digestion program is provided in Table 2. After the digestion, the samples were transferred to the 100 mL volumetric flask and diluted to 100 mL for further analysis. Details of the sample digestion were described by Li et al. (2014) [43].

2.5. Determination Procedure

2.5.1. HR-ICP-MS

Following ignition, the instrument parameters were initially adjusted at the low-resolution mode to achieve optimal operating conditions (Table 3). Subsequently, the instrument was switched to the medium resolution mode, and the ion optics parameters were fine-tuned to ensure intact peak shape and maximum signal. Mass calibration was then performed, and the standard deviation (SD) value was checked against the previous calibration, with a criterion of less than 150. Once these steps were completed, the instrument was prepared for sample analysis. For detailed information on the HR-ICP-MS analysis procedure, refer to Zhao et al. (2024) [60].

2.5.2. ICP-CCT-MS

When the instrument was stabilized after ignition, the optimization procedure was carried out for the ICP-CCT-MS instrument. The collision gas flow was adjusted from 0 mL/min to 4 mL/min gradually. After a stabilization period of 30 min, the parameters listed in Table 4 were adjusted to maximize the signal of each element in the tuning solution. Following these adjustments, the instrument was ready for sample testing. For a comprehensive description of the ICP-CCT-MS analysis procedure, please refer to Li et al. (2014) [43].

3. Results and Discussion

3.1. HR-ICP-MS

3.1.1. Isotope Selection

Selenium has six natural isotopes with relative atomic masses of 74, 76, 77, 78, 80, and 82 [24,51,61,62]. These isotopes can be subject to various interferences during mass spectrometry analysis, which can be categorized into diatomic ion interferences, isobar interferences, and doubly charged ion interferences (Table 5).
Diatomic ion interferences in selenium determination primarily originate from argon. Argon is used as the cooling, auxiliary, and nebulizer gas in the experiment and produces a strong signal in the test system that is challenging to separate even at high resolution. This interference mainly affects the determination of 74Se, 76Se, 78Se, and 80Se.
Isobar interferences primarily impact 74Se, 76Se, 80Se, and82Se, which may be interfered with by 74Ge, 76Ge, 80Kr, and 82Kr, respectively. Although 74Ge can be separated from 74Se at a low resolution, 76Ge and 76Se have similar atomic masses and can only be separated at a very high resolution (resolution = 34,570 amu). However, achieving such a high resolution poses challenges in maintaining signal strength and instrument stability, thus compromising the accuracy and reliability of results. Common argon separation methods, such as cryogenic fractionation and pressure friction distillation, have efficient separation capabilities but are not entirely accurate, resulting in residual krypton gas in ultrapure argon gas. This krypton gas interferes with 80Se and 82Se, making it difficult to completely separate or eliminate this interference.
Doubly charged ion interferences in the determination of selenium in coal-bearing strata are mainly from the rare earth elements (such as Sm2+, Nd2+, Gd2+, and Dy2+, etc.). These interferences can typically be effectively separated at medium to high resolution.
Considering the low abundance of 74Se in nature and the difficulties in separating interferences for 74Se, 76Se, 78Se, 80Se, and 82Se, comprehensive consideration led to the selection of 77Se as the isotope for HR-ICP-MS analysis.

3.1.2. Mass Spectral Interference and Correction

The main interference of 77Se comes from the doubly charged ions of rare earth elements and BaO. Table 6 shows that these interferences can be effectively separated within the resolution range of 1867–2525 amu. Therefore, the medium resolution (resolution = 4000 amu) is chosen for determination, allowing for the separation of interfering ions from the elements to be measured without excessively weakening the signal (Figure 1).
The results obtained from the actual tests verified the previous theoretical analysis. Taking SRM 2685c as an example, test data for six Se isotopes were obtained in multiple resolution modes, which are recorded in detail in Table 7. Among them, the results for three isotopes, 74Se, 78Se, and 80Se, are all below the detection limit, while among the remaining three isotopes, 77Se performs particularly well and is in high agreement with the certified value (1.90 μg/g). Based on these results, it can be confirmed that the determination of 77Se by HR-ICP-MS at medium-resolution mode is practical and effective.

3.2. Results Comparison

The method detection limit (MDL) was determined by calculating three times the standard deviation of the 11 results. The MDL of HR-ICP-MS (0.805 μg/L) was found to be higher than that of ICP-CCT-MS (0.095 μg/L), indicating that the latter method offers better precision (Table 8).
With the relative error (RE) ranging from 0% to 8.28%, HR-ICP-MS provides higher accuracy than ICP-CCT-MS such that the RE was in the range of 1.58%–17.27% (Table 8). The relative standard deviations (RSDs) for HR-ICP-MS and ICP-CCT-MS were observed to range from 5.82% to 8.37% and 4.78% to 9.97%, respectively (Table 9). The internal standard recoveries for HR-ICP-MS and ICP-CCT-MS were found to be in the range of 71.01%–84.56% and 86.56%–119.46%, respectively (Table 9). The lower recoveries obtained from HR-ICP-MS suggest weaker stability when compared to ICP-CCT-MS.
The detailed results of 10 consecutive runs of the standard reference material NIST 2685c using HR-ICP-MS and ICP-CCT-MS are listed in Table 10, and the X(bar)—S control charts are plotted accordingly. From Figure 2A,B, no anomalies are found during the consecutive tests for both HR-ICP-MS and ICP-CCT-MS, indicating that the process itself is stable and controlled. However, for both the X(bar) control charts and S control charts, ICP-CCT-MS has a larger range of fluctuations, suggesting that HR-ICP-MS demonstrates greater stability when a large number of samples are measured consecutively.
The results of the selected coal-bearing strata obtained from HR-ICP-MS and ICP-CCT-MS are generally consistent (Table 11). The internal standard recoveries of ICP-CCT-MS were superior to those of HR-ICP-MS, indicating that ICP-CCT-MS offers better instrumental stability.
HR-ICP-MS takes less time (25 ms) than ICP-CCT-MS (30 ms) to test a single sample while testing more cycles with similar results, giving it an advantage in testing a large number of consecutive samples.

4. Conclusions

This study presented an improved method for the determination of Se in coal-bearing strata using HR-ICP-MS. By selecting 77Se as the isotope for analysis and performing the measurement at medium resolution (resolution = 4000 amu), the results obtained from standard reference samples demonstrated close agreement with certified values. This approach proves to be reliable for Se determination in coal-bearing strata, as indicated by the low relative error. HR-ICP-MS exhibits superior stability in continuous determination, albeit with slightly weaker internal standard recovery. In addition, HR-ICP-MS offers the advantages of short test duration, and high accuracy, making it more suitable for the determination of Se in coal-bearing strata.

Author Contributions

Conceptualization, S.Z.; methodology, S.Z., R.J. and Q.H.; formal analysis, S.Z., K.T. and J.F.; data curation, Q.H. and N.S.; writing—original draft preparation, S.Z.; writing—review and editing, S.Z. All authors have read and agreed to the published version of the manuscript.

Funding

This research was supported by the National Key Research and Development Program of China (No. 2021YFC2902003) and the National Natural Science Foundation of China (No. 42272194).

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

The authors would like to thank Yan Wang and Qiuhao Pi from the China University of Mining and Technology (Beijing) for their great help in the analysis of the standard reference materials by the ICP-CCT-MS.

Conflicts of Interest

The authors declare no conflict of interest.

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Minerals 14 00510 g001
Figure 1. Peak of 77Se at low, medium, and high resolution. At low-resolution mode, the peak of the interferences overlaps with the peak of 77Se. At medium-resolution mode, the peak of the interferences is completely separated from the peak of 77Se. At high-resolution mode, the complete separation is also achieved, but the signal is strongly attenuated.
Figure 1. Peak of 77Se at low, medium, and high resolution. At low-resolution mode, the peak of the interferences overlaps with the peak of 77Se. At medium-resolution mode, the peak of the interferences is completely separated from the peak of 77Se. At high-resolution mode, the complete separation is also achieved, but the signal is strongly attenuated.
Minerals 14 00510 g001
Minerals 14 00510 g002
Figure 2. X(bar)—S control charts of NIST 2685c using HR-ICP-MS (A) and ICP-CCT-MS (B).
Figure 2. X(bar)—S control charts of NIST 2685c using HR-ICP-MS (A) and ICP-CCT-MS (B).
Minerals 14 00510 g002
Table 1. Overview of the investigated samples.
Table 1. Overview of the investigated samples.
Sample IDLithologyDescription
SRM 1632eBituminous coalNIST Standard reference material
SRM 2685c
SRM 1633cCoal fly ash
SRM 2691
GSR-20Carbonaceous-siliceous shaleNIM standard reference material
QS-9-1Bituminous coalNo.9 Coal Seam from Qisheng Mine, Xingtai Coal field, China (this study)
QS-9-2
QS-9-3
QS-9-4
QS-9-5
QS-9-RRoof, silty sandstoneQisheng Mine, Xingtai Coal field, China (this study)
QS-9-6MCarbonaceous mudstone
QS-9-7M
QS-9-8M
QS-9-FFloor, mudstone
Table 2. Microwave program for sample digestion. Modified from Li et al. (2014) [43].
Table 2. Microwave program for sample digestion. Modified from Li et al. (2014) [43].
StepTime (min)Temp (°C)Pressure (bar)Microwave Power (W)
18601001500
2121251001500
3151601301500
4152401601500
5602401601500
Cooling time60
Table 3. Optimized instrumental parameters for HR-ICP-MS.
Table 3. Optimized instrumental parameters for HR-ICP-MS.
ItemsValuesItemsValues/Status
Plasma RF power1380 WSpray chamber temperature3 ± 0.1 °C
Nebulizer gas pressure37.8 PSINebulizerTeflon neb
Auxiliary gas flow0.8 L/minPeristaltic pump speed30 RPM
Coolant gas flow13 L/minDwell time5 ms
Number of cycles5 timesTesting time for each run25 ms
Table 4. Optimized instrumental parameters for ICP-CCT-MS. After Li et al. (2014) [43].
Table 4. Optimized instrumental parameters for ICP-CCT-MS. After Li et al. (2014) [43].
ItemsValuesItemsValues/Status
Plasma RF power1400 WNebulizer Teflon neb
Nebulizer gas flow1.00 L/minCollision gas flow4 mL/min
Auxiliary gas flow0.8 L/minPeristaltic pump speed30 RPM
Coolant gas flow13.0 L/minDwell time10 ms
Number of main runs3 timesTesting time for each run30 ms
Table 5. Interference table of natural isotopes of Selenium.
Table 5. Interference table of natural isotopes of Selenium.
IsotopeMassAbundance (%)Major Interference
74Se73.922480.8774Ge; 148Sm2+; 148Nd2+; 38Ar36Ar
76Se75.919219.1276Ge; 152Sm2+; 152Gd2+; 38Ar2; 40Ar36Ar
77Se76.919917.50154Sm2+; 154Gd2+; 154BaO2+
78Se77.9177323.61156Gd2+; 156Dy2+; 156CeO2+; 40Ar38Ar
80Se79.9165249.9680Kr; 160Gd2+; 160Dy2+; 40Ar2
82Se81.916718.8482Kr; 164Dy2+; 164Er2+
Table 6. Interference table of 77Se.
Table 6. Interference table of 77Se.
InterferentMass Required Resolution (amu)
77Se76.91991
154Sm2+76.961111867
154Gd2+76.960441898
154BaO2+76.950362525
Table 7. Observed values (μg/g) of the six Se isotopes in the standard reference sample SRM 2685c of the HR-ICP-MS at different resolutions.
Table 7. Observed values (μg/g) of the six Se isotopes in the standard reference sample SRM 2685c of the HR-ICP-MS at different resolutions.
Detection Mode74Se76Se77Se78Se80Se82Se
Low Resolutionbdl10.592.18bdlbdl3.75
Medium Resolutionbdl9.891.94bdlbdl3.02
High Resolutionbdl9.511.86bdlbdl3.01
bdl, below detection limit.
Table 8. Selected elements, calibration curves, and method detection limits (MDLs) of HR-ICP-MS and ICP-CCT-MS.
Table 8. Selected elements, calibration curves, and method detection limits (MDLs) of HR-ICP-MS and ICP-CCT-MS.
InstrumentLinearity(μg/L)Correlation CoefficientMDL(μg/L)
HR-ICP-MS0–1000.9999460.805
ICP-CCT-MS0–1000.9999610.519
Table 9. Certified (Cer) and observed (Obs) values of Se (μg/g) in the standard reference samples, as well as relative error (RE, %), relative standard deviation (RSD, %), and the internal standard recovery (Rec, %) of the HR-ICP-MS and ICP-CCT-MS.
Table 9. Certified (Cer) and observed (Obs) values of Se (μg/g) in the standard reference samples, as well as relative error (RE, %), relative standard deviation (RSD, %), and the internal standard recovery (Rec, %) of the HR-ICP-MS and ICP-CCT-MS.
Sample ID HR-ICP-MSICP-CCT-MS
CerObsRERSDRecObsRERSDRec
SRM 1632e1.531.540.658.3792.871.561.964.78119.46
SRM 2685c1.901.942.107.1893.441.931.586.67113.81
SRM 1633c13.9013.324.178.1571.3616.3017.275.5398.16
SRM 269117.0017.784.596.9271.0116.652.069.9794.28
GSR-2029.731.586.335.8274.0434.2415.296.8098.33
Table 10. Observed values of Se (μg/g) and standard deviation (SD) for each cycle in the 10 consistent runs of the standard reference material NIST 2685c by HR-ICP-MS and ICP-CCT-MS.
Table 10. Observed values of Se (μg/g) and standard deviation (SD) for each cycle in the 10 consistent runs of the standard reference material NIST 2685c by HR-ICP-MS and ICP-CCT-MS.
Run 1Run 2Run 3Run 4Run 5Run 6Run 7Run 8Run 9Run 10Ave
HR-ICP-MS
Cycle 12.151.862.171.992.002.182.101.752.142.15
Cycle 21.922.131.771.801.671.681.842.042.061.81
Cycle 31.891.891.752.022.032.051.681.881.731.87
Cycle 41.751.881.972.111.972.142.141.961.931.90
Cycle 51.952.042.141.851.971.701.872.002.021.95
Ave1.931.961.961.951.931.951.931.931.971.941.94
SD0.130.100.180.110.130.220.170.100.140.110.14
ICP-CCT-MS
Cycle 12.102.021.962.102.121.941.941.761.961.84
Cycle 21.941.901.761.861.841.802.061.982.161.88
Cycle 31.741.882.141.861.942.101.881.761.562.16
Ave1.931.931.951.941.971.951.961.831.891.961.93
SD0.150.060.160.110.120.120.070.100.250.140.13
Table 11. Observed (Obs) values of Se (μg/g) and the internal standard recovery (Rec, %) of the selected coal-bearing strata samples by HR-ICP-MS and ICP-CCT-MS.
Table 11. Observed (Obs) values of Se (μg/g) and the internal standard recovery (Rec, %) of the selected coal-bearing strata samples by HR-ICP-MS and ICP-CCT-MS.
Sample IDHR-ICP-MSICP-CCT-MS
ObsRSDRecObsRSDRec
QS-9-11.984.3775.342.0217.48105.25
QS-9-23.185.2882.683.1223.56107.04
QS-9-39.972.7280.8410.288.67108.21
QS-9-46.683.5977.756.468.64105.76
QS-9-55.442.1679.985.685.15107.40
QS-9-R3.736.0270.593.6314.36113.44
QS-9-6M6.067.6577.626.1414.56112.89
QS-9-7M3.523.1478.443.808.33110.45
QS-9-8M2.963.7171.923.0515.14110.92
QS-9-F2.164.3975.642.2817.71108.78
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Zhao, S.; Jia, R.; Han, Q.; Shang, N.; Teng, K.; Feng, J. Comparison of the Application of High-Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS) and Collision/Reaction Cell Technology of Inductively Coupled Plasma Mass Spectrometry (ICP-CCT-MS) in the Determination of Selenium in Coal-Bearing Strata. Minerals 2024, 14, 510. https://doi.org/10.3390/min14050510

AMA Style

Zhao S, Jia R, Han Q, Shang N, Teng K, Feng J. Comparison of the Application of High-Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS) and Collision/Reaction Cell Technology of Inductively Coupled Plasma Mass Spectrometry (ICP-CCT-MS) in the Determination of Selenium in Coal-Bearing Strata. Minerals. 2024; 14(5):510. https://doi.org/10.3390/min14050510

Chicago/Turabian Style

Zhao, Shumao, Rongkun Jia, Qiuchan Han, Niande Shang, Kaiyan Teng, and Jiawei Feng. 2024. "Comparison of the Application of High-Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS) and Collision/Reaction Cell Technology of Inductively Coupled Plasma Mass Spectrometry (ICP-CCT-MS) in the Determination of Selenium in Coal-Bearing Strata" Minerals 14, no. 5: 510. https://doi.org/10.3390/min14050510

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